Water → Stavudine

HRID 988757노트

반응식

HRID 988757 반응식
[CH3:1][C:2]1[C:8](=[O:9])[NH:7][C:5](=[O:6])[N:4]([C@@H:10]2[O:14][C@H:13]([CH2:15][OH:16])[CH:12]=[CH:11]2)[CH:3]=1.CC(N(C)C)=O.O>C(O)(C)C>[CH3:1][C:2]1[C:8](=[O:9])[NH:7][C:5](=[O:6])[N:4]([C@@H:10]2[O:14][C@H:13]([CH2:15][OH:16])[CH:12]=[CH:11]2)[CH:3]=1

참가 물질

4

반응물 2

HCID 962WaterHCID 11722976Stavudine DMA

생성물 1

HCID 18283Stavudine수율 91.4%

시약·촉매·용매 1

HCID 3776Isopropanol용매

반응 조건

온도
70 °C

실험 절차

The Stavudine-DMA solvate (15.22 g, 0.0489 mole), water (5.5 g) and isopropanol (150 mL) were combined and heated to about 70° C. when all solids had dissolved to give a clear colourless solution, heating was continued so as to distill the solution at atmospheric pressure until about 35 mL of isopropanol remained. The solution was allowed to cool on its own with agitation and a mass of crystals formed after 20 minutes. The mixture was 10 placed on an ice-water bath for I hour, filtered, washed with isopropanol (2×11 mL) and air dried overnight to give 10.02 g (0.0447 mole, 91.4%) of pure white crystalline Stavudine. The HPLC results are given in Table 2.

후처리

  1. dissolutionhad dissolved
  2. customto give a clear colourless solution
  3. temperatureheating
  4. distillationto distill the solution at atmospheric pressure until about 35 mL of isopropanol
  5. temperatureto cool on its own with agitation
  6. customa mass of crystals formed after 20 minutes
  7. customplaced on an ice-water bath for I hour
  8. filtrationfiltered
  9. washwashed with isopropanol (2×11 mL) and air
  10. customdried overnight

출처 및 근거

ORD 기록
ord-e8f3c82148cf40ab81e188ca35401372
출처 데이터셋
uspto-grants-2003_10
특허 번호
US06635753B1

반응 노트

불러오는 중…